CN103224829B - Special cleaning fire-resistant oil and preparation method thereof - Google Patents
Special cleaning fire-resistant oil and preparation method thereof Download PDFInfo
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Abstract
The present invention is directed to a special cleaning fire-resistant oil and preparation method thereof, which comprises the components of base oil trixylenyl phosphate, tricresyl phosphate and di- (tert-butyl phenyl) phenyl phosphate at weight ratio of (0.5-0.8):(1.2-1.5):(1.1-1.13), 0.9 wt% of epoxy soybean oil isooctyl phenyl, 0.4wt% of benzotriazole and 0.6wt%-1.5 wt% of EDTA. The medium and high voltage resistant oil provided by the present invention has characteristics of low chlorine content and acid value, high ignition point and boiling point, and advantages of good lubricity, abrasion resistance, aging resistance, anti-foam, anti-flammability and thermal stability etc. The conditioning system used in large generating units of more than 300MW is a reliable working system to guarantee the safe operation of generating units, and the products not only can be applied in high-temperature, high-pressure and hydraulic lubrication systems, but also can be extended to other systems of high-temperature heat source or near the open flame.
Description
Technical field
The invention belongs to fire resistant oil field, especially a kind of special fire resistant oil and preparation method thereof that cleans.
Background technology
KR series fire resistant lubricant is to aim at high temperature, high pressure or have the high-performance fire resistant oil using under naked light Working environment, this product is to be basic material from ISOPROPYL PHENYL DIPHENYL PHOSPHATE, and in addition other auxiliary agent modulation forms, be widely used in generating, lubricated and the hydraulic efficiency system of metallurgy and main equipment, also can be used for military project and aviation field.Wherein KR-99-G(high pressure) and KR-99-Z(in press) fire resistant oil is the dedicated hydraulic fire resistant oil for the height of automobile generating unit, pressure speed governing and Controlling System, the use temperature that KR-99-G and KR-99-Z fire resistant oil have is high, operating pressure is large, spontaneous ignition temperature is high, resistivity is high, and lubricity is good, good cooling results, the advantages such as rapid heat dissipation are the ideal products of replace imported fire resistant oil.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art part, a kind of special fire resistant oil and preparation method thereof that cleans is provided, this fire resistant oil has that cl content is low, acid number is low, spontaneous ignition temperature and the high characteristic of boiling point, there is good oilness, resistance to abrasion, resistance to deterioration, anti-spumescence, the advantages such as non-flame properties and heat-resistant quality energy.
The technical scheme that the present invention realizes object is as follows:
The special fire resistant oil of a kind of cleaning, its component comprises:
Base oil trixylyl phosphate: Tritolyl Phosphate: weight ratio=0.5-0.8:1.2 ~ 1.5:1.1 ~ 1.13 of two (tert-butyl-phenyl) phenyl phosphate ester, then add the epoxy soybean oil monooctyl ester of 0.9wt%, the benzotriazole of 0.4wt%, the EDTA of 0.6wt%-1.5wt%.
A preparation method who cleans special fire resistant oil, method is as follows:
(1) qualified base oil trixylyl phosphate: Tritolyl Phosphate: two (tert-butyl-phenyl) phenyl phosphate ester by weight: mixture is carried out in 0.5-0.8::1.2 ~ 1.5:1.1 ~ 1.13, and fully stirs 2.5 hours;
(2) in getting (1), mixture oil product is put into dry, clean constant volume device and is added by joining oil product quantity, adds 0.9% epoxy soybean oil, adds 0.4% phenylpropyl alcohol three nitrogen files, and the EDTA of 0.6%-1.5%, fully stirs into mother liquor, and temperature is controlled at 60 ± 2 DEG C;
(3) (1) the (2) mother liquor completing is added in still, fully stirs 65 ± 2 DEG C of temperature controls, balance 3 ~ 5 o'clock;
(4) (3) will filtering through 50-60 mesh sieve of completing, temperature is controlled at 65 ± 2 DEG C, balance 14 ~ 16 o'clock;
(5) (4) do total analysis through sampling what complete, qualified, become the finished product.
And the production method of described Tritolyl Phosphate is:
Adopt stock yard p-cresol and phosphorus oxychloride in proportion: 2.2-2.6:1-1.3 is esterification under the effect of catalyzer calcium magnesium composite catalyst, the M-and P-cresols that catalyst levels is 0.22-0.3wt%, acid discharge; 145 DEG C of neutral equilibrium temperature controls, underpressure distillation 730-750mmHg left and right, 380-390 DEG C, then rectification and purification 730-750mmHg, 380-390 DEG C, filters 50-60 order and filters, and getting its fine work is base oil.
In the middle of it, the requirement of p-cresol Non-scale.
And the preparation method of described trixylyl phosphate is as follows:
Adopt raw material xylenol and phosphorus oxychloride in molar ratio: 2.2-2.6:1-1.3 is esterification under the effect of catalyzer calcium magnesium composite catalyst, the xylenol that catalyst levels is 0.22wt%-0.3wt%, acid discharge; 145 DEG C of neutral equilibrium temperature controls, underpressure distillation: 720-750mmHg, 380-410 DEG C, then rectifying: 720-750mmHg, 400-410 DEG C of purification, then the filtration of 50-60 order, getting its fine work is base oil.
And the production method of described two or two (tert-butyl-phenyl) phenyl phosphate ester (TBPP) is as follows:
Adopt raw material p-tert-butylphenol, phenol and phosphorus oxychloride, according to a certain percentage: 2:4:3, esterification under the effect of catalyzer calcium magnesium composite catalyst, the p-tert-butylphenol that catalyst levels is 0.15wt%, temperature is controlled at 120-150 DEG C, acid discharge, neutral equilibrium, underpressure distillation 740-755mmHg, 390-400 DEG C, rectifying 740-755mmHg again, 390-400 DEG C of purification, filters 50-60 order and filters, and getting its fine work is base oil.
And the preparation method's of described calcium magnesium composite catalyst step is as follows:
(1) claim HZSM-5 type molecular sieve, calcium sulfate, magnesium chloride, sesbania powder, in the reactor adding water to;
(2) stir, heat, control temperature of reaction at 80 ± 5 DEG C, heating 6 ~ 8h;
(3) reaction product is filtered, suction filtration, washes with water;
(4) the product after washing is dried, grind, get≤100 object catalyzer, roasting, obtains calcium magnesium composite catalyst;
Raw material weight umber is than as follows:
Advantage of the present invention and beneficial effect are:
1, to have cl content low for middle high-pressure fire resistant oil provided by the invention, and acid number is low, and the characteristic that spontaneous ignition temperature and boiling point are high has good oilness, resistance to abrasion, resistance to deterioration, anti-spumescence, the advantages such as non-flame properties and heat-resistant quality energy.For the adjusting system of the above Generator Set of 300MW, a kind of reliable work solution matter that ensures generating set safe operation, this product application, in industry high temperature, high pressure, oil pumping systems such as metallurgy, machinery, military projects, also extends near the system of working other high temperature heat source or naked light.
2, preparation method of the present invention is simple, process control is easy, and acid number is easily controlled, and the product indices of producing is all high compared with currently available products.
Embodiment
Below in conjunction with embodiment, following embodiment is illustrative, is not determinate, can not limit protection scope of the present invention with following embodiment.
The special fire resistant oil of a kind of cleaning, its component comprises:
Trixylyl phosphate (TXP): Tritolyl Phosphate (TCP): weight ratio=0.5-0.8:1.2 ~ 1.5:1.1 ~ 1.13 of two (tert-butyl-phenyl) phenyl phosphate ester (TBPP), then add the epoxy soybean oil monooctyl ester of 0.9wt%, the benzotriazole of 0.4wt%, the EDTA of 0.6wt%-1.5wt%.
The preparation method of above-mentioned fire resistant oil is as follows:
(1) qualified base oil trixylyl phosphate (TXP) Tritolyl Phosphate (TCP): two (tert-butyl-phenyl) phenyl phosphate ester (TBPP) is carried out mixture, and fully stirred 2.5 hours by weight=0.5-0.8::1.2 ~ 1.5:1.1 ~ 1.13;
(2) in getting (1), mixture oil product is put into dry, clean constant volume device and is added by joining oil product quantity, adds 0.9% epoxy soybean oil, adds 0.4% phenylpropyl alcohol three nitrogen files, and the EDTA of 0.6%-1.5%, fully stirs into mother liquor, and temperature is controlled at 60 ± 2 DEG C;
(3) (1) the (2) mother liquor completing is added in still, fully stirs 65 ± 2 DEG C of temperature controls, balance 3 ~ 5 o'clock;
(4) (3) will filtering through 50-60 mesh sieve of completing, temperature is controlled at 65 ± 2 DEG C, balance 14 ~ 16 o'clock;
(5) (4) do total analysis through sampling what complete, qualified, become the finished product; Be packaged as processed oil with cleaning-drying pail pack afterwards and weigh, warehouse-in.
The production method of its raw material is as follows:
1, the production method of described Tritolyl Phosphate is:
Adopt stock yard p-cresol and phosphorus oxychloride in proportion: 2.2-2.6:1-1.3 is esterification under the effect of catalyzer calcium magnesium composite catalyst, the M-and P-cresols that catalyst levels is 0.22-0.3wt%, acid discharge; 145 DEG C of neutral equilibrium temperature controls, underpressure distillation 730-750mmHg left and right, 380-390 DEG C, then rectification and purification 730-750mmHg, 380-390 DEG C, filters 50-60 order and filters, and getting its fine work is base oil.
2, the preparation method of described trixylyl phosphate is as follows:
Adopt raw material xylenol and phosphorus oxychloride in molar ratio: 2.2-2.6:1-1.3 is esterification under the effect of catalyzer calcium magnesium composite catalyst, the xylenol that catalyst levels is 0.22wt%-0.3wt%, acid discharge; 145 DEG C of neutral equilibrium temperature controls, underpressure distillation: 720-750mmHg, 380-410 DEG C, then rectifying: 720-750mmHg, 400-410 DEG C of purification, then the filtration of 50-60 order, getting its fine work is base oil.
3, the production method of described two (tert-butyl-phenyl) phenyl phosphate ester (TBPP) is as follows:
Adopt raw material p-tert-butylphenol, phenol and phosphorus oxychloride, according to a certain percentage: 2:4:3, esterification under the effect of catalyzer calcium magnesium composite catalyst, the p-tert-butylphenol that catalyst levels is 0.15wt%, temperature is controlled at 120-150 DEG C, acid discharge, neutral equilibrium, underpressure distillation 740-755mmHg, 390-400 DEG C, rectifying 740-755mmHg again, 390-400 DEG C of purification, filters 50-60 order and filters, and getting its fine work is base oil.
4, the preparation method's of described calcium magnesium composite catalyst step is as follows:
(1) claim HZSM-5 type molecular sieve, calcium sulfate, magnesium chloride, sesbania powder, in the reactor adding water to;
(2) stir, heat, control temperature of reaction at 80 ± 5 DEG C, heating 6 ~ 8h;
(3) reaction product is filtered, suction filtration, washes with water;
(4) the product after washing is dried, grind, get≤100 object catalyzer, roasting, obtains calcium magnesium composite catalyst.
Table 1 cleans the technical requirements of special fire resistant oil
| Index name | KR-99 | KR-99-G |
| Acid number: ㎎ KOH/g≤ | 0.080 | 0.070 |
| Density: 20c g/cm 3 | 1.130～1.170 | 1.130～1.170 |
| Boiling point: DEG C >= | 235 | 240 |
| Pour point: DEG C≤ | -18 | -18 |
| Kinematic viscosity: 40 DEG C of mm 2/s | 28.8～35.5 | 37.9～44.3 |
| Moisture content: PPM≤ | 1000 | 1000 |
| Granularity: AEA-60 level≤ | 6 | 4 |
| Nature point: DEG C (triangle is also) >= | 530 | 530 |
| DEG C (hot plate) >= | 700 | 700 |
| Chlorinity: %(w/w) >= | 0.005 | 0.005 |
| Foam property, the high ml of foam≤ | 90 | 25 |
| 20 DEG C of Ω cm of resistivity >= | 5.0×10 9 |
Table 2 Tritolyl Phosphate quality and technical index
| Project | Index |
| Color and luster (Pt-Co) # ≤ | 80 |
| 20 DEG C of g/cm of density 3 ≤ | 1.180 |
| Acid number mgKOH/g≤ | 0.080 |
| 40 DEG C of mm of viscosity 2/s ≥ | 30 |
| Flash-point DEG C >= | 225 |
| Spontaneous ignition temperature DEG C >= | 430 |
| Cl content mg/g≤ | 35 |
Table 3 two (tert-butyl-phenyl) phenyl phosphate ester quality and technical index
| Project | Index |
| Color and luster (Pt-Co) # ≤ | 80 |
| 20 DEG C of g/cm of density 3 ≤ | 1.170 |
| Acid number mgKOH/g≤ | 0.080 |
| 40 DEG C of mm of viscosity 2/s ≥ | 45 |
| Flash-point DEG C >= | 235 |
| Spontaneous ignition temperature DEG C >= | 530 |
| Cl content mg/g≤ | 50 |
Table 4 trixylyl phosphate quality and technical index
| Project | Index |
| Color and luster (Pt-Co) # ≤ | 100 |
| 20 DEG C of g/cm of density 3 ≤ | 1.140 |
| Acid number mgKOH/g≤ | 0.070 |
| 40 DEG C of mm of viscosity 2/s ≥ | 60 |
| Flash-point DEG C >= | 230 |
| Spontaneous ignition temperature DEG C >= | 430 |
| Cl content mg/g≤ | 25 |
Claims (6)
1. clean a special fire resistant oil, it is characterized in that: consist of the following composition:
Base oil trixylyl phosphate: Tritolyl Phosphate: the weight ratio=0.5-0.8:1.2-1.5:1.1-1.13 of two (tert-butyl-phenyl) phenyl phosphate ester, then add the epoxy soybean oil monooctyl ester of 0.9wt%, the benzotriazole of 0.4wt%, the EDTA of 0.6wt%-1.5wt%.
2. a preparation method for the special fire resistant oil of cleaning as claimed in claim 1, is characterized in that: method is as follows:
(1) qualified base oil trixylyl phosphate: Tritolyl Phosphate: two (tert-butyl-phenyl) phenyl phosphate ester by weight: 0.5-0.8:1.2-1.5:1.1-1.13 carries out mixture, and fully stir;
(2) getting in (1) mixture oil product puts into dry, clean constant volume device and adds by joining oil product quantity, add the epoxy soybean oil monooctyl ester of 0.9wt%, add the benzotriazole of 0.4wt%, the EDTA of 0.6wt%-1.5wt%, fully stir into mother liquor, temperature is controlled at 60 ± 2 DEG C;
(3) (2) mother liquor completing is added in (1) still, fully stirs 65 ± 2 DEG C of temperature controls, balance 3～5 hours;
(4) (3) that complete will be filtered through 50-60 mesh sieve, temperature is controlled at 65 ± 2 DEG C, balance 14～16 hours;
(5) (4) that complete are done to total analysis through sampling, qualified, become the finished product.
3. the preparation method of the special fire resistant oil of cleaning according to claim 2, is characterized in that: the production method of described Tritolyl Phosphate is:
Adopt stock yard, p-cresol and phosphorus oxychloride in proportion: 2.2-2.6:1-1.3 is esterification under the effect of catalyzer calcium magnesium composite catalyst, between catalyst levels is 0.22-0.3wt%, p-cresol, acid discharge; 145 DEG C of neutral equilibrium temperature controls, underpressure distillation 730-750mmHg, 380-390 DEG C, then rectification and purification 730-750mmHg, 380-390 DEG C, 50-60 order filters, and getting its fine work is base oil.
4. the preparation method of the special fire resistant oil of cleaning according to claim 2, is characterized in that: the preparation method of described trixylyl phosphate is as follows:
Adopt raw material xylenol and phosphorus oxychloride in molar ratio: 2.2-2.6:1-1.3 is esterification under the effect of catalyzer calcium magnesium composite catalyst, the xylenol that catalyst levels is 0.22wt%-0.3wt%, acid discharge; 145 DEG C of neutral equilibrium temperature controls, underpressure distillation: 720-750mmHg, 380-410 DEG C, then rectifying: 720-750mmHg, 400-410 DEG C of purification, then the filtration of 50-60 order, getting its fine work is base oil.
5. the preparation method of the special fire resistant oil of cleaning according to claim 2, is characterized in that: the production method of described two (tert-butyl-phenyl) phenyl phosphate ester is as follows:
Adopt raw material p-tert-butylphenol, phenol and phosphorus oxychloride, according to a certain percentage: 2:4:3, esterification under the effect of catalyzer calcium magnesium composite catalyst, catalyst levels is the p-tert-butylphenol of 0.15wt%, temperature is controlled at 120-150 DEG C, acid discharge, neutral equilibrium, underpressure distillation 740-755mmHg, 390-400 DEG C, then rectifying 740-755mmHg, 390-400 DEG C of purification, 50-60 order filters, and getting its fine work is base oil.
6. according to the preparation method of the special fire resistant oil of cleaning described in claim 3 or 4 or 5, it is characterized in that: the preparation method's of described calcium magnesium composite catalyst step is as follows:
(1) claim HZSM-5 type molecular sieve, calcium sulfate, magnesium chloride, sesbania powder, add water in reactor;
(2) stir, heat, control temperature of reaction at 80 ± 5 DEG C, heating 6～8h;
(3) reaction product is filtered, suction filtration, washes with water;
(4) product after washing is dried, grind, get≤100 object catalyzer, roasting, obtains calcium magnesium composite catalyst;
Raw material weight umber is as follows:
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| CN114181757B (en) * | 2020-09-14 | 2022-06-28 | 安美科技股份有限公司 | A kind of phosphate ester fire-resistant oil |
| CN113956928A (en) * | 2021-10-27 | 2022-01-21 | 中国石油化工股份有限公司 | Phosphate ester hydraulic oil cleaning composition and preparation method thereof |
| CN116240064B (en) * | 2023-03-17 | 2024-09-13 | 安徽中天石化股份有限公司 | High-annealing detergency hydraulic oil and preparation method and application thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1231458A (en) * | 1967-09-06 | 1971-05-12 | ||
| CN102695785A (en) * | 2009-11-12 | 2012-09-26 | 吉坤日矿日石能源株式会社 | Flame-retardant hydraulic oil composition |
| CN103013635A (en) * | 2012-12-27 | 2013-04-03 | 安陆市奥森石油化学有限责任公司 | Ester type fire-resistant hydraulic fluid and preparation method thereof |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1231458A (en) * | 1967-09-06 | 1971-05-12 | ||
| CN102695785A (en) * | 2009-11-12 | 2012-09-26 | 吉坤日矿日石能源株式会社 | Flame-retardant hydraulic oil composition |
| CN103013635A (en) * | 2012-12-27 | 2013-04-03 | 安陆市奥森石油化学有限责任公司 | Ester type fire-resistant hydraulic fluid and preparation method thereof |
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